This study reports the use of 19F MRS to study halothane in the brain of eight patients recovering from halothane anesthesia of short duration. Resonances attributable to halothane were observed up to 90 min after withdrawal of the anesthetic agent. The signal-to-noise ratio for an unlocalized spectrum acquired using a 6 cm surface coil was typically 20 with data collection times of 2 min. In seven patients a single resonance was seen with a mean (±SD) chemical shift of +43.3 (±1.8) ppm, referenced to NaF at 0 ppm. This resonance exhibited a T1 value of between 0.5 and 1 s, and a T2* (estimated from the linewidth of the resonance) between 3.5 and 10 ms. In one patient two resonances were observed with chemical shifts of +38 and +41 ppm. Because we cannot exclude the possibility that this was due to field inhomogeneity, the significance of the last finding is uncertain. However, phantom studies show that the chemical shift of halothane in different environments (such as water, olive oil, methanol, and lecithin) can vary to an extent that accounts for the two resonances seen in our patient. These results demonstrate the feasibility of in vivo19F MRS studies of fluorinated volatile agents in humans. The potential for clinical 19F MRS of fluorinated anesthetics is discussed.